Beta-diketo mono imine vanadium olefinic polymerization catalyst, and its preparing method and use

A diketone monoimine vanadium olefin and polymerization catalyst technology, which is applied in the field of β-diketone monoimine vanadium olefin polymerization catalyst and preparation, and can solve the problems of low catalytic activity, easy deactivation, poor high temperature resistance, etc.

Inactive Publication Date: 2006-10-25
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the shortcomings of low catalytic activity, easy deactivation, and poor high temperature resistan

Method used

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  • Beta-diketo mono imine vanadium olefinic polymerization catalyst, and its preparing method and use
  • Beta-diketo mono imine vanadium olefinic polymerization catalyst, and its preparing method and use
  • Beta-diketo mono imine vanadium olefinic polymerization catalyst, and its preparing method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 4.00 g of acetylacetone, equivalent to 40 mmol, 4.85 g of 2,6-dimethylaniline, equivalent to 40 mmol, 15 mL of methanol, and 1 mL of formic acid into a dry 100 mL reaction flask, and heat to reflux for 24 hours. The solvent methanol was distilled off with a rotary evaporator, and petroleum ether containing 1% ethyl acetate was used as eluent, and the residue was subjected to column chromatography to obtain 4.15 g of white solid Schiff's base, with a yield of 51%. According to mass spectrometry, the molecular ion peak m / e is 203. Elemental analysis found values: C, 76.92%; H, 8.39%; N, 6.85%; theoretical value (C13H17NO): C, 76.81%; H, 8.43%; N, 6.89%.

[0035] Under a nitrogen atmosphere, add 0.406 g of the above-obtained Schiffer’s base (equivalent to 2.0 mmol) and 20 mL of anhydrous tetrahydrofuran into a dry 100 mL reaction flask, stir at room temperature for 10 min, and cool to -78°C. Within 5 minutes, 1.375 mL of a 1.60 mol / L n-butyllithium hexane solution, equi...

Embodiment 2

[0037] With 7.09g of 2,6-diisopropylaniline, which is equivalent to 40mmol, to replace 2,6-dimethylaniline in Example 1, the experimental operation is the same as in Example 1, and 4.77g of white solid Schiffer’s base is obtained. rate 46%. According to mass spectrometry, the molecular ion peak m / e is 259. Elemental analysis measured values: C, 78.61%; H, 9.68%; N, 5.44%; theoretical value (C17H25NO): C, 78.72%; H, 9.71%; N, 5.40%.

[0038] 0.52g of Schiff's base prepared in Example 2, equivalent to 2mmol, replaced the Schiff's base obtained in Example 1, and the experimental operation was the same as in Example 1 to obtain 0.51g of brown β-diketone monoimine vanadium olefin polymerization catalyst, Yield 49%. According to mass spectrometry, the molecular ion peak m / e is 524. Elemental analysis found values: C, 57.09%; H, 7.65%; N, 2.64%; theoretical value (C25H40Cl2NO3V): C, 57.26%; H, 7.69%; N, 2.67%.

Embodiment 3

[0040] Add 5.19g of 1-phenyl-1,3-butanedione, equivalent to 32mmol, 5.96g of aniline, equivalent to 64mmol, 15mL of methanol, and 1mL of formic acid into a dry 100mL reaction flask, heat and reflux for 36h, and cool the reaction solution. A colorless solid precipitated out. Filter, wash with cold petroleum ether for several times, and dry in vacuo to obtain 3.95 g of white solid Schiff's base with a yield of 52%. According to mass spectrometry, the molecular ion peak m / e is 237. Elemental analysis found values: C, 80.62%; H, 6.36%; N, 5.86%; theoretical value (C16H15NO): C, 80.98%; H, 6.37%; N, 5.90%.

[0041] 0.47g of Schiff's base prepared in Example 3, equivalent to 2mmol, replaced the Schiff's base obtained in Example 1, and the experimental operation was the same as in Example 1 to obtain 0.45g of brown β-diketone monoimine vanadium olefin polymerization catalyst, Yield 45%. Mass spectrometry, the molecular ion peak m / e is 502. Elemental analysis found values: C, 57.1...

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Abstract

The invention discloses a beta-diketone mono-imide vanadium olefinic polymerization catalyst and the manufacture method and the application of ethylene polymerizing, ethylene and norborene polymerizing, ethylene and alpha-alkene or norborene copolymerization. Under the catalysis of formic acid, beta-diketone compound and aniline or the ramification of aniline taking condensation reaction in methanol solution to gain Schiff base; under the non water and non oxygen condition, the Schiff base taking reaction with butyl lithium to gain negative ion ligand; under the non-water, non oxygen condition, the negative ion ligand taking coordination reaction with VCl3, the beta-ketimine vanadium alkene polymerization catalyst could be gained. The invention could catalyze ethylene polymerization, and the copolymerizing of ethylene and alpha-alkene or norborene.

Description

technical field [0001] The invention relates to a β-diketone monoimine vanadium olefin polymerization catalyst and a preparation method. [0002] The present invention also relates to the application of the β-diketone monoimine vanadium olefin polymerization catalyst in catalyzing ethylene polymerization, ethylene and norbornene copolymerization, ethylene and α-olefin copolymerization. Background technique [0003] In the 1950s, Ziegler and Natta each discovered that transition metal β-diketone monoimide vanadium olefin polymerization catalysts could catalyze olefin polymerization under mild conditions. In the following fifty years, a lot of research has emerged to develop A transition metal catalyst system with high activity and high control over product structure. At the same time, the continuous renewal of polyolefin products has brought revolutionary changes to people's lives, and they are increasingly widely used in industry, agriculture, national defense, transportati...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/64
Inventor 李悦生唐丽明段轶群张贵宝李彦国陈学思刘靖宇
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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